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Sodium Hydroxide → 2,5-Dimethyl-4-hydroxy-tetrahydrofuran-3-one

HRID 1578019
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HRID 1578019 반응식
[CH3:1][CH:2]1[CH:6]([OH:7])[CH:5]([OH:8])[CH:4]([CH3:9])[O:3]1.[OH-].[Na+]>[Ag].O>[CH3:1][CH:2]1[C:6](=[O:7])[CH:5]([OH:8])[CH:4]([CH3:9])[O:3]1
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참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 204869562,5-Dimethyl-3,4-dihydroxy-tetrahydrofuran

생성물 1

HCID 103131462,5-Dimethyl-4-hydroxy-tetrahydrofuran-3-one

시약·촉매·용매 2

HCID 23954Silver촉매2회HCID 962Water용매2회

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온도
20 °C

실험 절차

A vertical tubular reactor of 2 cm internal diameter, at the top of which 28 g of silver crystals (8 g of particles with diameters from 0.75 to 1 mm, 14 g of particles with diameters of from 0.4 to 0.75 mm and 6 g of particles with diameters of from 0.2 to 0.4 mm) were arranged, as a 2 cm thick bed, above a silver gauze screen, was fed, per hour, with a gaseous mixture, at 175° C., of 18.7 liters of 2,5-dimethyl-3,4-dihydroxy-tetrahydrofuran (=110 g), 72 liters of air and 100 liters of nitrogen. The catalyst temperature was 535° C. and the residence time over the catalyst about 0.04 second. After having passed over the catalyst, the gas mixture was immediately cooled to 20° C. by passing it into water. The resulting solution was brought to pH 8 with 10% strength NaOH solution. The water was then stripped off at 20 mbar and the residue was distilled at 1.3 mbar. This gave, at 61°-66° C., 35 g of a distillate containing about 80% of 2,5-dimethyl-4-hydroxy-tetrahydrofuran-3-one, and, at 109°-120° C., 60 g of unconverted 2,5-dimethyl-3,4-dihydroxy-tetrahydrofuran. The conversion was about 45% and the yield, based thereon, about 70%.

후처리

  1. customwas 535° C.
  2. customover the catalyst about 0.04 second
  3. distillationthe residue was distilled at 1.3 mbar
  4. additionThis gave, at 61°-66° C., 35 g of a distillate containing about 80% of 2,5-dimethyl-4-hydroxy-tetrahydrofuran-3-one
  5. customat 109°-120° C.

출처 및 근거

ORD 기록
ord-1d66bdba6f4a4d46adeba42813aa99c3
출처 데이터셋
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04290960

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